Dispersive micron-sized strip-shaped polyamide material as well as preparation method and application thereof

Abstract

The embodiment of the invention relates to the technical field of polyamide material synthesis, and particularly discloses a dispersive micron-sized strip-shaped polyamide material as well as a preparation method and application thereof, and the dispersive micron-sized strip-shaped polyamide material comprises the following raw materials: polyamide plastic, a poor solvent and a proper amount of NaOH aqueous solution. According to the embodiment of the invention, by reasonably using the raw materials and adopting a reasonable preparation process, the shape and size of the polyamide material can be accurately controlled, and the polyamide material with specific shape and size distribution is obtained; the problem that polyamide particles with specific forms and size distribution are difficult to obtain in an existing polyamide production process is solved. Moreover, the preparation method provided by the embodiment of the invention is simple, effectively expands the development space of the polyamide material in some high-performance application fields, and has a wide market prospect.

Description

Technical Field

[0001] The embodiment of the present invention belongs to the technical field of polyamide material synthesis, and specifically relates to a dispersed micron-sized strip polyamide material and a preparation method and application thereof. Background Art

[0002] With the continuous development of science and technology, more and more new materials are being developed and applied. Among them, polyamide, commonly known as nylon (PA), is a synthetic polymer engineering plastic that is widely used in textiles, automobiles, office supplies, electronics, packaging and other industries for its excellent mechanical properties, wear resistance, chemical resistance and good processing performance.

[0003] At present, the main varieties of common polyamide products on the market are PA1010, PA6, PA66, PA610, etc. In general, polyamide products belong to a class of polymer materials with strong polarity, and hydrogen bonds can be formed between molecules, so the melting temperature is high, and the melting temperature range is narrow, with a clear melting point, high strength, high toughness, heat resistance and oil resistance. However, the above-mentioned prior art solutions have the following defects: In the prior art, due to the characteristics of the molecular structure of polyamide, traditional synthesis methods are often difficult to obtain polyamide particles with specific morphology and size distribution, which limits its further development in certain high-performance application fields. Therefore, it is of great industrial value to develop a preparation method that can accurately control the morphology and size of polyamide particles. Summary of the invention

[0004] The purpose of the embodiments of the present invention is to provide a dispersed micron-sized strip polyamide material to solve the problem that the existing polyamide production process mentioned in the above background technology is often difficult to obtain polyamide particles with specific morphology and size distribution.

[0005] To achieve the above objectives, the embodiments of the present invention provide the following technical solutions:

[0006] A dispersible micron-sized strip polyamide material comprises the following raw materials: polyamide plastic, poor solvent, and an appropriate amount of alkaline aqueous solution or reducing agent aqueous solution; wherein the alkaline aqueous solution is an aqueous solution of one or more of ammonia, sodium hydroxide, potassium hydroxide, and calcium hydroxide, with a mass concentration of 0.1-20%. The reducing agent aqueous solution is citric acid, citric acid, sodium citrate, glucose, formaldehyde, etc., with a mass concentration of 0.1-20%. Preferably, it is a NaOH (sodium hydroxide) aqueous solution.

[0007] Preferably, the polyamide plastic is selected from polyamide 66.

[0008] Preferably, the poor solvent is selected from any one or more of ethylene glycol, glycerol, butanediol, etc. Preferably, ethylene glycol is used.

[0009] Another object of the embodiment of the present invention is to provide a method for preparing a dispersed micron-sized strip-shaped polyamide material, the method for preparing a dispersed micron-sized strip-shaped polyamide material comprising the following steps:

[0010] The polyamide plastic is weighed in proportion and added to a poor solvent, the polyamide plastic is completely dissolved at 170-197° C., then cooled to 140-160° C. and an alkaline aqueous solution or a reducing agent aqueous solution is added to mix evenly, then cooled to 115-155° C. for constant temperature incubation, and finally filtered, washed, and dried to obtain the dispersed micron-sized strip polyamide material.

[0011] Another object of the embodiment of the present invention is to provide a dispersed micron-sized strip-shaped polyamide material prepared by the above-mentioned preparation method.

[0012] Another object of an embodiment of the present invention is to provide an application of the above-mentioned dispersed micron-sized strip-shaped polyamide material in the preparation of polymer materials.

[0013] Compared with the prior art, the embodiments of the present invention have the following beneficial effects:

[0014] The dispersed micron-sized strip polyamide material provided by the embodiment of the present invention can accurately control the morphology and size of polyamide product particles through the reasonable use of polyamide plastics, poor solvents, and an appropriate amount of alkaline aqueous solution or reducing agent aqueous solution, and adopt a reasonable preparation process to obtain nylon particles with specific morphology and size distribution, effectively expanding its development space in certain high-performance application fields, and solving the problem that the existing polyamide production process is often difficult to obtain polyamide particles with specific morphology and size distribution. Moreover, the preparation method of the dispersed micron-sized strip polyamide material provided by the embodiment of the present invention is simple, can be used to prepare other types of polymer materials, and has broad market prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present invention.

[0016] Figure 1 This is a scanning electron microscope micrograph of the dispersed micron-sized strip-shaped polyamide material provided in one embodiment of the present invention.

[0017] Figure 2 This is a scanning electron microscope micrograph of a dispersed micron-sized strip-shaped polyamide material provided by another embodiment of the present invention.

[0018] Figure 3This is a scanning electron microscope micrograph of a dispersed micron-sized strip-shaped polyamide material provided by another embodiment of the present invention.

[0019] Figure 4 This is a scanning electron microscope micrograph of a dispersed micron-sized strip-shaped polyamide material provided by another embodiment of the present invention.

[0020] Figure 5 This is a scanning electron microscope micrograph of a dispersed micron-sized strip-shaped polyamide material provided by another embodiment of the present invention. DETAILED DESCRIPTION

[0021] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in combination with the embodiments of the present invention and the accompanying drawings. Obviously, the following embodiments will help those skilled in the art to further understand the embodiments of the present invention, but do not limit the embodiments of the present invention in any form. It should be pointed out that for those of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the embodiments of the present invention. These all belong to the protection scope of the embodiments of the present invention.

[0022] The specific implementation of the present invention is described in detail below in conjunction with specific embodiments.

[0023] An embodiment of the present invention provides a dispersible micron-sized strip-shaped polyamide material, and the dispersible micron-sized strip-shaped polyamide material includes the following raw materials:

[0024] Polyamide plastic, poor solvent, and an appropriate amount of alkaline aqueous solution or reducing agent aqueous solution; wherein the mass concentration of the alkaline aqueous solution or reducing agent aqueous solution is 0.1-20%.

[0025] In the embodiments of the present invention, polyamide is commonly known as nylon, and its English name is Polyamide (PA), which is a general term for polymers containing amide groups in the macromolecular main chain repeating units. Polyamide can be prepared by ring-opening polymerization of lactam, or by polycondensation of diamine and dibasic acid. Polyamide plastics are polyamide products developed on the basis of polyamide fibers, and their main varieties include polyamide 6, polyamide 46, polyamide 56, polyamide 66, polyamide 11, polyamide 12, polyamide 610, polyamide 612, polyamide 1010, etc. Among them, polyamide 6 and polyamide 66 have the highest output, accounting for more than 90% of polyamide output; polyamide 11 and polyamide 12 have outstanding low-temperature toughness; polyamide 46, also known as polybutylene adipamide, commonly known as nylon 46, referred to as PA46, is an aliphatic polyamide formed by the condensation of butanediamine and adipic acid. Although it has a similar molecular structure to nylon 66, PA46 has more amide groups on each given length of chain and a more symmetrical chain structure. It has developed rapidly due to its excellent heat resistance.

[0026] In the embodiments of the present invention, by adopting a reasonable preparation process, the morphology and size of nylon particles can be accurately controlled to obtain nylon particles with specific morphology and size distribution, effectively expanding its development space in certain high-performance application fields.

[0027] As another preferred embodiment of the present invention, the mass concentration of the alkaline aqueous solution or the reducing agent aqueous solution is 0.5-2%.

[0028] As another preferred embodiment of the embodiment of the present invention, specifically, in the embodiment of the present invention, the polyamide plastic is selected from polyamide 66.

[0029] As another preferred embodiment of the present invention, in the raw material of the dispersed micron-sized strip-shaped polyamide material, 0.01-5 wt % of polyamide plastic is added to every 100 ml of poor solvent.

[0030] As another preferred embodiment of the present invention, in the raw material of the dispersed micron-sized strip-shaped polyamide material, 0.05-2 wt % of polyamide plastic is added to every 100 ml of poor solvent.

[0031] As another preferred embodiment of the present invention, the poor solvent is selected from any one or more of ethylene glycol, glycerol, butylene glycol, ethanol, acetone, dimethylformamide, chloroethanol, propylene glycol and the like.

[0032] As another preferred embodiment of the present invention, the poor solvent is selected from any one or more of ethylene glycol, glycerol, butanediol, etc. A further preferred poor solvent is selected from ethylene glycol.

[0033] The embodiment of the present invention also provides a method for preparing a dispersed micron-sized strip-shaped polyamide material, specifically a method for preparing a dispersed micron-sized strip-shaped polyamide by a specific synthesis process, the method comprising the following steps:

[0034] The polyamide plastic is weighed in proportion and added to a poor solvent, and the polyamide plastic is completely dissolved at 170-197° C., then cooled to 140-160° C. and an alkaline aqueous solution or a reducing agent aqueous solution is added to mix evenly, and then cooled to 115-155° C. for constant temperature incubation, and finally filtered, washed, and dried to obtain the dispersed micron-sized strip polyamide material.

[0035] The method for preparing the dispersed micron-sized strip-shaped polyamide material provided in the embodiment of the present invention can accurately control the morphology of nylon particles to meet the needs of specific applications.

[0036] As another preferred embodiment of the present invention, in the method for preparing the dispersed micron-sized strip-shaped polyamide material, the temperature is lowered to 120-150° C. and incubated at a constant temperature for 5 min-12 h.

[0037] Preferably, the preparation method of the dispersed micron-sized strip polyamide material is to add 0.05-2wt% of polyamide 66 plastic to 100 ml of ethylene glycol poor solvent, heat it in an oil bath to 170-200°C and keep it for 5-120 minutes to completely dissolve it, then cool it to 160-140°C, add 5mL-40ml of NaOH aqueous solution (mass concentration is 0.1-10%) and continue to cool it to 150-120°C and incubate it at a constant temperature for 1min-12h, then cool it to room temperature, filter it, wash it, and dry it to obtain the dispersed micron-sized strip polyamide material.

[0038] Further preferably, the method for preparing the dispersed micron-sized strip-shaped polyamide material comprises the following steps:

[0039] 1) Add 0.05-2wt% of polyamide 66 to 100 ml of ethylene glycol poor solvent.

[0040] 2) Heat the oil bath to 170-197°C and maintain for 5-120 minutes to completely dissolve it.

[0041] 3) When the temperature drops to 160-140°C, add 5mL-40ml of NaOH aqueous solution (mass concentration is 0.1-20%).

[0042] 4) Continue to cool down to 150-120℃ and incubate at a constant temperature for 5 minutes to 12 hours.

[0043] 5) After completion, the mixture is cooled to room temperature, filtered, washed and dried to obtain the dispersed micron-sized strip-shaped polyamide material.

[0044] The embodiment of the present invention further provides a dispersed micron-sized strip-shaped polyamide material prepared by the above-mentioned method for preparing the dispersed micron-sized strip-shaped polyamide material.

[0045] The embodiment of the present invention also provides an application of the above-mentioned dispersed micron-sized strip polyamide material in the preparation of polymer materials, such as the preparation of polymer materials such as rubber, fiber, and plastic. Among them, the plastic can be a thermoplastic plastic, and the main thermoplastic plastics include polyethylene, polypropylene, polystyrene, polymethyl methacrylate, polyvinyl chloride, nylon, polycarbonate, polyurethane, polytetrafluoroethylene, polyethylene terephthalate, etc.; it can also be a thermosetting plastic, and the common ones include epoxy resin, phenolic plastic, polyimide, melamine formaldehyde resin, etc. It is especially suitable for dispersed micron-sized strip polymer materials.

[0046] The technical effects of the dispersed micron-sized strip polyamide material of the embodiment of the present invention are further described below by listing specific embodiments.

[0047] Example 1

[0048] A dispersed micron-sized strip polyamide material, the preparation method of which specifically comprises the following steps:

[0049] 1. Add 0.5wt% polyamide 66 to 100ml ethylene glycol.

[0050] 2. Heat the oil bath to 190°C and maintain for 40 minutes to allow it to completely dissolve.

[0051] 3. When the temperature drops to 150°C, add 20 ml of NaOH aqueous solution (mass concentration is 0.5%).

[0052] 4. Continue to cool down to 140℃ and incubate for 3 hours.

[0053] 5. After completion, cool to room temperature, filter, wash and dry to obtain dispersed strip-shaped polyamide 66.

[0054] In this embodiment, in order to verify that the prepared dispersed strip polyamide 66 is a dispersed micron-sized strip polyamide material, a dispersed strip polyamide 66 sample is subjected to a scanning electron microscope test, and the obtained scanning electron microscope micrograph is as shown in FIG. Figure 1 As shown. Figure 1 It can be seen that the scale is 10 microns, and the prepared dispersed strip polyamide 66 is in the form of dispersed strips with a size of about 10 microns.

[0055] Example 2

[0056] A dispersed micron-sized strip polyamide material, the preparation method of which specifically comprises the following steps:

[0057] 1. Add 1.5wt% polyamide 66 to 100ml ethylene glycol.

[0058] 2. Heat the oil bath to 195°C and maintain for 30 minutes to allow it to completely dissolve.

[0059] 3. When the temperature drops to 160°C, add 10 ml of vitamin C aqueous solution (mass concentration is 2%).

[0060] 4. Continue to cool down to 130℃ and incubate for 8 hours.

[0061] 5. After completion, cool to room temperature, filter, wash and dry to obtain dispersed strip-shaped polyamide 56.

[0062] In this embodiment, in order to verify that the prepared dispersed strip polyamide 66 is a dispersed micron-sized strip polyamide material, a dispersed strip polyamide 66 sample is subjected to a scanning electron microscope test, and the obtained scanning electron microscope micrograph is as shown in FIG. Figure 2 As shown. Figure 2 It can be seen that the scale is 10 microns, and the prepared dispersed strip polyamide 66 is in the form of dispersed strips with a size of about 10 microns.

[0063] Example 3

[0064] Compared with Example 1, except that the mass concentration of the NaOH aqueous solution is 0.1%, other aspects are the same as Example 1.

[0065] The dispersed strip polyamide 66 sample was subjected to scanning electron microscopy test, and the obtained scanning electron microscope micrograph was as follows Figure 3 As shown. Figure 3 It can be seen that the scale is 10 microns, and the prepared dispersed strip polyamide 66 is in a dispersed strip state with a size of about 10 microns.

[0066] Example 4

[0067] Compared with Example 1, except that the mass concentration of the NaOH aqueous solution is 2%, other aspects are the same as Example 1.

[0068] The dispersed strip polyamide 66 sample was subjected to scanning electron microscopy test, and the obtained scanning electron microscope micrograph was as follows Figure 4 As shown. Figure 4 It can be seen that the scale is 10 microns, and the prepared dispersed strip polyamide 66 is in a dispersed state with a size of about 10 microns, with a small amount of accumulation.

[0069] Example 5

[0070] Compared with Example 1, except that the mass concentration of the NaOH aqueous solution is 20%, the others are the same as Example 1.

[0071] The dispersed strip polyamide 66 sample was subjected to scanning electron microscopy test, and the obtained scanning electron microscope micrograph was as follows Figure 5 As shown. Figure 5 It can be seen that the scale is 10 microns, and the prepared dispersed strip polyamide 66 is in a dispersed state with a size of about 10 microns. A small amount of PA66 strips are dispersed in small islands.

[0072] Example 6

[0073] Compared with Example 1, except that the added amount of polyamide 66 is 0.01wt%, the other aspects are the same as Example 1.

[0074] The prepared samples are dispersed strips with a width of about 1 micron and a length of about 10 microns. The ends and edges of the strips are thinner and are evenly dispersed in the field of view.

[0075] Example 7

[0076] Compared with Example 1, except that the added amount of polyamide 66 is 0.05wt%, the other aspects are the same as Example 1.

[0077] The prepared sample is a dispersed strip with a width of about 10 microns and a length of about 30 microns, and the strip structure is relatively thick and dispersed in the field of view.

[0078] Example 8

[0079] Compared with Example 1, except that the added amount of polyamide 66 is 2 wt %, the other aspects are the same as Example 1.

[0080] The prepared sample is a dispersed strip with a width of about 10 microns and a length of about 30 microns, and the strip structure is relatively thick and dispersed in the field of view.

[0081] Example 9

[0082] Compared with Example 1, except that the added amount of polyamide 66 is 5wt%, the other aspects are the same as Example 1.

[0083] The prepared sample is a dispersed strip with a width of about 2 microns and a length of about 10 microns, and the ends of the strip structure are thicker and dispersed in the field of view.

[0084] According to the above results, it can be seen that the dispersed micron-sized strip polyamide material provided by the embodiment of the present invention can accurately control the morphology and size of the polyamide product particles through the reasonable use of polyamide plastics, poor solvents and an appropriate amount of alkaline aqueous solution or reducing agent aqueous solution, and adopt a reasonable preparation process to obtain polyamide particles with specific morphology and size distribution. These polyamide particles have excellent mechanical properties and thermal stability, and can be widely used in various industrial fields, especially in applications requiring high-performance nylon particles, effectively expanding its development space in certain high-performance application fields, and solving the problem that the existing polyamide production process is often difficult to obtain polyamide particles with specific morphology and size distribution. Moreover, the preparation method of the dispersed micron-sized strip polyamide material provided by the embodiment of the present invention is simple, can be used to prepare other types of polymer materials, and has broad market prospects.

[0085] Finally, it should be noted that the polyamide 56, polyamide 66, etc. in the embodiment of the present invention are all products of existing manufacturers. For example, in this embodiment, polyamide 66 can specifically adopt the polyamide 66 product of model PA66 produced by Asahi Chemical Corporation of Japan. The above are all conventional production raw materials, which can be selected according to specific needs, and will not be described in detail here.

[0086] The above is a detailed description of the preferred embodiments of the present invention, describing the basic principles, main features and advantages of the present invention. However, those skilled in the art should understand that the embodiments of the present invention are not limited to the above embodiments. The above embodiments and descriptions are only preferred examples of the present invention and are not intended to limit the present invention. Various changes can be made within the knowledge of ordinary technicians in this field without departing from the purpose of the embodiments of the present invention. It is not necessary and impossible to list all the embodiments here. The obvious changes or modifications derived from this are still within the scope of protection of the embodiments of the present invention.

Claims

1. A dispersed micron-sized strip polyamide material, characterized in that: The dispersed micron-sized strip polyamide material includes the following raw materials: polyamide plastic, poor solvent, and an appropriate amount of one or more alkaline aqueous solutions or reducing agent aqueous solutions; wherein the alkaline aqueous solution is one or more aqueous solutions of ammonia, sodium hydroxide, potassium hydroxide, and calcium hydroxide; and the reducing agent aqueous solution is one or more aqueous solutions of vitamin C, citric acid, sodium citrate, glucose, and formaldehyde.

2. The dispersed micron-sized strip polyamide material according to claim 1, characterized in that: The mass concentration of the alkaline aqueous solution or the reducing agent aqueous solution is 0.5-20%.

3. The dispersed micron-sized strip polyamide material according to claim 2, characterized in that: The polyamide plastic is selected from any one of polyamide 56, polyamide 66, polyamide 11, and polyamide 610.

4. The dispersed micron-sized strip polyamide material according to claim 3, characterized in that: In the raw material of the dispersed micron-sized strip polyamide material, 0.01-5wt% of polyamide plastic is added to every 100 ml of poor solvent.

5. The dispersed micron-sized strip polyamide material according to claim 4, characterized in that: In the raw material of the dispersed micron-sized strip polyamide material, 0.05-2 wt % of polyamide plastic is added to every 100 ml of poor solvent.

6. The dispersed micron-sized strip polyamide material according to claim 5, characterized in that: The poor solvent is selected from any one or more of ethylene glycol, glycerol, and butanediol.

7. A method for preparing the dispersed micron-sized strip polyamide material according to any one of claims 1 to 6, characterized in that: The following steps are involved: The polyamide plastic is weighed in proportion and added to a poor solvent, the polyamide plastic is completely dissolved at 170-197° C., then the temperature is lowered to 140-160° C. and one or more alkaline aqueous solutions or reducing agent aqueous solutions are added to mix evenly, then the temperature is lowered to 115-155° C. for constant temperature incubation, and finally filtered, washed, and dried to obtain the dispersed micron-sized strip polyamide material.

8. The method for preparing the dispersed micron-sized strip polyamide material according to claim 7, characterized in that: In the preparation method of the dispersed micron-sized strip polyamide material, the constant temperature incubation time is 5 minutes to 12 hours.

9. A dispersed micron-sized strip-shaped polyamide material prepared by the preparation method according to claim 7.

10. Use of the dispersed micron-sized strip polyamide material as claimed in claim 1 or 2 or 3 or 4 or 5 or 6 or 9 in the preparation of polymer materials.

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